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Clayton, Anthony Brian. "Photopolymerised urethane acrylates /." Title page, contents and summary only, 1992. http://web4.library.adelaide.edu.au/theses/09PH/09phc622.pdf.
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Trenor, Scott Russell. "Synthesis and Characterization of Tailored Photoactive Macromolecules." Diss., Virginia Tech, 2004. http://hdl.handle.net/10919/27314.
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Coumarin and cinnamate derivatives were positioned as either polymer chain ends or side groups to synthesize photoactive macromolecules and gain the ability to reversibly control molecular weight and crosslink density using UV light. The cinnamates and coumarins were reacted onto the polymers via multiple reaction pathways. Polymers were functionalized with coumarin or cinnamate groups via an esterification reaction between hydroxyl functionalities and an acid chloride derivatized coumarin group. In addition to the esterification reaction, cinnamates were also coupled to polymers via a ring opening reaction between a hydroxyl functionalized cinnamate derivative and a maleic anhydride repeat unit copolymerized into the polymer. Both functional groups undergo a [2p + 2p] photodimerization reaction (coumarin groups in the UVA and cinnamate groups in the UVB), which was utilized to crosslink and chain-extend macromolecules. Coumarin dimers possess the additional ability to photocleave and thus reverse when irradiated at 254 nm.
The coumarin reversible photodimerization reaction was utilized to reversibly increase the molecular weight and molecular weight distribution of coumarin-functionalized PEG monols and diols. For example, the number average molecular weight of the coumarin-functionalized PEG diol doubled and the
molecular weight distribution increased from 1.08 to 2.75 when exposed to 110 J cm-2 of UVA irradiation. Subsequent photocleavage (UVC irradiation, 2 J cm-2) of the chain-extended PEGs, cleaved coumarin dimers decreasing the molecular weight and molecular weight distribution to their original values.
A number of poly(alkyl acrylate) and poly(methyl acrylate) systems were functionalized with coumarin groups to study the effect of the glass transition temperature and alkyl ester side group composition on the photodimerization reaction and subsequent crosslinking. The glass transition temperature (Tg) acted as an on/off switch for the photodimerization reaction. While the absolute difference between Tg and irradiance temperature did not affect the rate or extent of photodimerization reaction, polymers with a Tg greater than the irradiance temperature displayed less reaction than those with a Tg lower than the irradiance temperature. The final extent of conversion was controlled by a complex combination of factors including alkyl ester side chain steric bulkiness. Coumarin-functionalized alkyl acrylates based on ethylhexyl acrylate were tested as detachable PSAs. A 98% decrease in the adhesive peel strength was observed after exposure to UVA irradiation.
Cinnamate groups were utilized in the design and synthesis of UV-curable hot melt pressure sensitive adhesives (PSAs). The cinnamate groups were attached to the PSAs to provide a method to increase molecular weight and add a small amount of crosslinking leading to an increase the adhesive strength of the PSAs. Broadband UV irradiation from a laboratory scale industrial lamp increased the peel strength of the adhesives. Postcure of the irradiated cinnamate-functionalized UV-curable hot melt PSAs was reduced compared to photoinitiated free-radical photocurable UV-curable hot melt PSAs.Ph. D.
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Lessard, Benoît H. 1985. "Random controlled free radical copolymerization of acrylic acidstyrene and tert-butyl acrylatestyrene mixtures using nitroxide mediators." Thesis, McGill University, 2008. http://digitool.Library.McGill.CA:80/R/?func=dbin-jump-full&object_id=111944.
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Controlled free radical polymerization facilitates the production of polymers with highly defined microstructures like traditional ionic polymerization; but in contrast allows for previously unattainable monomer combinations such as acrylic acid in its non-protected form. Incorporation of acrylic acid into styrene was done by random copolymerization of acrylic acid (directly and in its protected form as tert-butyl acrylate) with styrene. Styrene/tert-butyl acrylate (S/t-BuA) as well as styrene/acrylic acid (S/AA) mixtures were copolymerized to form tapered or gradient copolymers. Using an alkoxyamine unimolecular initiator, 2-[N- tert-butyl-2,2-(dimethylpropyl)aminooxy] propionic acid (BlocBuilder RTM), along with additional free nitroxide (SG1), the effect of acid protection on polymerization kinetics and copolymer composition was determined. Adding 4.5 mol% SG1/BlocBuilderRTM greatly improved the control of S/t-BuA copolymerization with low polydispersities (1.14-1.22) whereas the S/AA required higher levels of SG1 to produce polymers with low polydispersities that were comparatively still broader compared to the S/t-BuA system (polydispersities ∼ 1.3-1.4 at 9 mol% SG1/BlocBuilderRTM). S/AA copolymerization required higher SG1 concentrations to compensate for degradation of SG1 by attack from the acrylic acid monomer.
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Evans, Stacy Alexandria Banford. "Dithiafulvene (1,3-dithiole) and acrylate liquid crystals: Synthesis of monomers and polymers with possible electronic and electro-optic applications, and investigations in the synthesis of pure (meth)acrylates." Diss., The University of Arizona, 1989. http://hdl.handle.net/10150/184777.
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In this work, using the idea of an electrically conducting "functional unit," monomers and polymers with possible electronic and electro-optic applications were synthesized. The synthesis and polymerizations were, in many cases, novel and non-trivial. Dithiafulvene (1,3-dithiole) and variations of this functional unit were synthesized and incorporated into new condensation polymers. Polyesters, polyamides and polyhydrazones were all successfully synthesized and could be cast into films. These new polymers might be applicable as processable conducting materials if compatible dopants are employed or by themselves in the area of third order non-linear optics. Using a (meth)acrylate backbone, a spacer group of six methylene units, and a phenyl-CO₂-phenyl mesogen, linked by an ester group to a strongly polar optically active center containing a methoxy group, three new novel monomers and polymers were designed to exhibit smectic C* liquid-crystal phases. The polymers exhibited liquid crystalline behavior as was shown in differential scanning calorimetry and optical microscopy. Further studies and investigations in the synthesis of pure (meth)acrylate esters and their homopolymers yielded surprising results with regard to the Schotten-Baumann reaction. Interestingly, the use of meth(acryloyl) chloride in this scheme leads to (meth)acrylic anhydride, which is not easily isolable from distillable products. This anhydride is responsible for gelation in the polymerization of glycolate esters, and cannot be removed by work-up with various nucleophiles without disrupting desired ester functions. An S(N)2 method is recommended in this work.
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Mange, Siyabonga. "Synthesis, polymerisation and characterisation of a novel olefin-modified acrylate monomer, 1-methyl-1-propyl-hexel acrylate." Thesis, Stellenbosch : Stellenbosch University, 2005. http://hdl.handle.net/10019.1/50459.
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Thesis (PhD)--Stellenbosch University, 2005.ENGLISH ABSTRACT: Finding use for byproducts from the chemical industry holds many advantages for a country's economy. Synthesis of new monomers from such byproducts adds value to otherwise otherwise low-value material. The synthesis of a new olefin-modified acrylate monomer, 1-methyl-1-propyl-hexyl acrylate (1-MPHA), derived from 1-pentene, is reported. Homopolymerisation of the monomer 1-MPHA was carried out in both benzene and in toluene. The products of full-conversion of the homopolymer poly-(1-MPHA) were characterised by GPC, NMR, TGA and DMA. Kinetic studies of the homopolymerisation process of 1- MPHAwere also undertaken. The monomer 1-methyl-1-propyl-hexyl acrylate (1-MPHA) was copolymerised with methyl methacrylate (MMA). Samples obtained from full conversion copolymerisations at various 1-MPHAIMMAfeed ratios were characterised by GPC, NMR, TGA and DMA. Reactivity ratios of the two monomers were obtained from in situ 1H NMR kinetic studies. 1-MPHA was also copolymerised with vinyl acetate (VAc). Samples obtained from full conversion copolymerisation with a 1-MPHA content ranging from 2 to 16 wt% were characterised by GPC, NMR, TGA and DMA. The solubility parameter and the hydrophobicity of the VAc/1-MPHA copolymers were also determined. Reactivity ratios of the two monomers were obtained from in situ 1HNMR kinetic studies. Further copolymerisation studies with styrene and glycidyl methacrylate as comonomers were undertaken. The chemical analysis and thermogravimetric analysis of the copolymers are reported. In conclusion, the use of 1-methyl-1-propyl-hexyl acrylate as a comonomer results in a reduction in the glass transition temperature, better thermal stability, increased hydrophobicity with an insignificant loss in stiffness of the copolymers. These properties are due to the long and branched chain structure of the 1-MPHA monomer.
AFRIKAANSE OPSOMMING: Gebruik van byprodukte van die chemiese nywerheid hou groot voordele in vir die land se ekonomie. Sintese van nuwe monomere vanuit sulke byprodukte dra by tot waardetoevoeging tot andersins lae-waarde byprodukte. Die sintese van 'n nuwe olefien-gewysigde akrilaatmonomeer afkomstig van 1-penteen, naamlik 1-metiel-1-propiel-heksielakrilaat (1-MPHA), word hier beskryf. Homopolimerisasie van die monomeer 1-MPHA is uitgevoer in beide benseen en tolueen. Die produkte van die volledige omskakeling van die homopolimeer is met behulp van GPC, KMR, TGA en DMA gekarakteriseer. Die reaksiekinetika van die homopolimerisasie van 1-MPHA is ook ondersoek. Die monomeer 1-MPHA is met metielmetakrilaat (MMA) gekopolimeriseer. Monsters van die volledig omgeskakelde kopolimere met verskeie 1- MPHNMMA voerverhoudings is m.b.v. GPC, KMR,' TGA en DMA gekarakteriseer. Die reaktiwiteitsverhoudings van die twee monomere is vanaf 1HKMR-studies bepaat. 1-MPHA is ook met vinielasetaat (VAc) gekopolimeriseer. Monsters van die produk van die volledige kopolimerisasie met 1-MPHA , met 'n inhoud van 2- 16 massa 0/0, is ook m.b.v. GPC, KMR, TGA en DMA gekarakteriseer. Die 1- MPHA het die hidrofobisiteit van VAc/1-MPHA aansienlik verhoog. Die reaktiwiteitsverhoudings van die twee monomere is vanaf in situ 1H KMRstudies bepaal. Verdere kopolimerisasiestudies met stireen en glisidielmetakrilaat as komonomere is onderneem. Chemiese- en termogravimetriese analises van die kopolimere is gedoen en gerapporteer. Ter afsluiting, die gebruik van 1-metiel-1-propiel-heksielakrilaat as komonomeer het 'n verlaging in die glasoorgangstemperatuur, verhoogde termiesestabiliteit, verhoogde hidrofobisiteit, en 'n klein verlies in die stewigheid (Eng. stiffness) van die kopolimeer tot gevolg. Hierdie eienskappe is as gevolg van die lang, vertakte kettingstruktuur van die 1-MPHA monomeer.
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Sung, Jonggeun. "Design and synthesis of plant oil-based UV-curable acrylates for sustainable coating applications." Diss., Kansas State University, 2018. http://hdl.handle.net/2097/38657.
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Doctor of PhilosophyDepartment of Grain Science and Industry
X. Susan Sun
A demand in sustainable polymers has been increased because of the environment concerns and saving finite petroleum resources. Plant oils are promising renewable resources to produce environmentally friendly polymer applications. Soybean oil-based resins such as epoxidized soybean oil (ESO) and acrylated epoxidized soybean oil (AESO) have been well-known functionalized plant oils, but relatively low performances of their polymers and a competition with food production have been disadvantages. Thus, in this study, we designed new plant oil-based acrylates using non-food resources and achieved excellent properties of the acrylates for coatings and thermoset applications. Firstly, we developed coating materials with high mechanical, thermal and coating performances using acrylated epoxidized camelina oil (AECO) as a main acrylate monomer with various meth(acrylates) as reactive diluents Next, acrylated epoxidized cardanol modified fatty acids from camelina oil (AECFA) was successfully synthesized, and a phenolic structure with long aliphatic side chains with acrylic groups was obtained. The novel structure of AECFA provided rigidity into its polymer maintained with flexibility, and AECFA coating material showed better performances in terms of all properties such as mechanical, thermal, viscoelastic, and coating performances, as compared to commercial AESO resin. Finally, acrylated epoxidized allyl 10-undecenoate (AEAU) was developed from 10-undecenoic acid, castor oil derivative. The single fatty ester structure with di-functional acrylates of AEAU had very lower viscosity and showed better thermoset performances than those of triglyceride-based acrylates such as AESO and AECO. Thus, AEAU had a potential to an alternative to AESO for thermoset applications.
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Bagoury, Mohamed al. "Synthesis of aqueous polymer colloids based on saccharide monomers and alkyl acrylates through emulsion polymerization." [S.l. : s.n.], 2005. http://deposit.ddb.de/cgi-bin/dokserv?idn=974074527.
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Li, Peichun. "Synthesis of poly(ε-caprolactone) based copolymers in molten state by living polymerization." Saint-Etienne, 2009. http://www.theses.fr/2009STET4001.
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In this dissertation, we investigate the continuous synthesis of functional poly(ε-caprolactone) (PCL) and controlled copolymerization of ε-caprolactone (CL) with n-butyl acrylate (BA). In the first part, Ti[O(CH2)4OCH=CH2]4 was synthesized and used to obtain double-bond functionalized PCL. The kinetics of Ti[O(CH2)4OCH=CH2]4 initiated ring-opening polymerization (ROP) of ε-caprolactone was thoroughly investigated and the gelation process of CL/Ti[O(CH2)4OCH=CH2]4/BA/BPO system was monitored by rheological method. Then the cross-linked PCL/PBA networks were in situ synthesized in poly(methyl methacrylate) (PMMA) matrix via reactive extrusion. In the second part, Ti[OCH2CCl3]4 was synthesized and used as difunctional initiator for ROP of ε-caprolactone and atom transfer radical polymerization (ATRP) of n-butyl acrylate. The kinetics of Ti[OCH2CCl3]4 initiated ROP of ε-caprolactone and ATRP of n-butyl acrylate were evaluated. PCL-block-PBA copolymers were synthesized by sequential combination of ROP of ε-caprolactone and ATRP of n-butyl acrylate. Then PBA synthsized by Ti[OCH2CCl3]4 initiated ATRP was used as a macroinitiator, PCL-block-PBA copolymer was in situ polymerized in PMMA matrix in Haake internal mixer to investigate the possibility of producing well-defined in PCL-block-PBA copolymer in PMMA matrix through reactive extrusionDans cette thèse, nous étudions la synthèse de poly(ε-caprolactone) (PCL) fonctionnelle ainsi que la copolymérisation contrôlée de l'ε-caprolactone (CL) avec l'acrylate de butyle (BA) dans une matrice polymère thermoplastique via l'extrusion réactive. Dans la première partie, l'initiateur de formule Ti[O(CH2)4OCH=CH2]4 a été synthétisé dans le but d'élaborer de la PCL fonctionnelle. La cinétique de polymérisation par ouverture de cycle (ROP) initiée par Ti[O(CH2)4OCH=CH2]4 a été étudiée. Par ailleurs, un processus de gélification a été mis en évidence par rhéologie lors de la polymérisation simultanée de l'ε-caprolactone et de l'acrylate de butyle. Dans un second temps, ces réseaux ont été élaborés dans une matrice de poly (methyl methacrylate) (PMMA) par voie fondue. Dans la deuxième partie, un initiateur schématisé par Ti[OCH2CCl3]4 a été synthétisé dans le but de coupler 2 techniques de polymérisations contrôlées, à savoir la polymérisation par ROP de l'ε-caprolactone et la polymérisation radicalaire par transfert d'atomes (ATRP) de l'acrylate de butyle. Les cinétiques de polymérisation ont été évaluées et des copolymères PCL-bloc-PBA ont été élaborés. Parallèlement, un macro initiateur porteur de chaînes de polybutylacrylate a été synthétisé par ATRP à partir de Ti(OCH2CCl3)4. Ce dernier a permis d'élaborer un copolymère avec de l'ε-caprolactone dans une matrice PMMA en mélangeur interne. L'objectif de cette dernière partie étant de synthétiser, in situ et en voie fondue dans une matrice thermoplastique, un matériau de structure contrôlée afin d'améliorer les propriétés de la matrice
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Lee, Jehoon. "Synthesis, characterization, and applications of the low cross-link density poly acrylate elastomers using direct reversible addition fragmentation chain transfer cross-linker." University of Akron / OhioLINK, 2018. http://rave.ohiolink.edu/etdc/view?acc_num=akron149798302050725.
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Hinojosa, Barbara R. "Nanoparticles Engineered to Bind Serum Albumin: Microwave Assisted Synthesis, Characterization, and Functionalization of Fluorescently-Labeled, Acrylate-Based, Polymer Nanoparticles." Thesis, University of North Texas, 2010. https://digital.library.unt.edu/ark:/67531/metadc30466/.
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The potential use of polymeric, functionalized nanoparticles (NPs) as drug delivery vectors was explored. Covalent conjugation of albumin to the surface of NPs via maleimide chemistry proved problematic. However, microwave assisted synthesis of NPs was not only time efficient, but enabled the exploration of size control by changing the following parameters: temperature, microwave power, reaction time, initiator concentration, and percentage of monomer used. About 1.5 g of fluorescently-labeled, carboxylic acid-functionalized NPs (100 nm diameter) were synthesized for a total cost of less than $1. Future work will address further functionalization of the NPs for the coupling of albumin (or other targeted proteins), and tests for in vivo biodistribution.
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Lizotte, Jeremy Richard. "Synthesis and Characterization of Tailored Macromolecules via Stable Free Radical Polymerization Methodologies." Diss., Virginia Tech, 2003. http://hdl.handle.net/10919/28998.
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The stable free radical polymerization methodology for production of controlled macromolecules was investigated using a novel monomer, 2-vinylnaphthalene. Initial polymerizations resulted in molecular weight distributions typical of conventional free radical polymerization techniques (>2.0). Manipulation of the initiator concentration and the molar ratio of initiator to nitroxide demonstrated no significant control over the resulting polymer products. Analysis of the polymerization kinetics for a 2-vinylnaphthalene polymerization performed in the presence and absence of the free radical initiator revealed identical monomer consumption profiles as well as pseudo first order kinetics indicating a significant degree of the thermal polymerization was occurring at the polymerization temperature (130°C). Comparison of the thermal polymerization propensity of 2-vinylnaphthalene and styrene revealed an increased tendency for 2-vinylnapthahlene to undergo thermal polymerization. Styrene is considered highly active in its propensity to thermally polymerize. However, an Arhenius analysis using in situ FTIR was employed to determine the activation energy for the thermal polymerization of styrene and 2-vinylnaphthalene. The 2-vinylnaphthalene activation energy for thermal polymerization was determined for the first time to be almost 30 kJ/mol less than styrene. A novel modified Mayo mechanism was proposed for the 2-vinylnaphthalene thermal initiation mechanism. Moreover, this thermal initiation was employed to initiate nitroxide mediated polymerizations of styrene. This first use of a 2-vinylnaphthalene initiating system resulted in polystyrene with a large macrocyclic initiating fragment. The presence of the initiating moiety was studied using both UV-Vis spectroscopy and 1H NMR spectroscopy.
The extension of stable free radical polymerization to the acrylate monomer family was examined using a novel nitroxide mediator, N-tert-butyl-N-[1-diethylphosphono-(2,2-dimethylpropyl)] nitroxide (DEPN). The synthesis of DEPN was monitored using in situ FTIR spectroscopy to determine optimum reaction conditions. The purified nitroxide was subsequently employed in the synthesis of various block and random acrylate copolymers. The production of a unique amphiphilic block copolymer consisting of acrylic sequences was achieved. Poly(t-butyl acrylate-b-2ethylhexyl acrylate-b-t-butyl acrylate) was synthesized using the SFRP process. The t-butyl functionalities were subsequently removed in a post-polymerization acid catalyzed hydrolysis. The effect of steric bulk and electronic factors on the resulting SFRP process was also investigated and revealed similar polymerization kinetics for various alkyl acrylates. However, addition of a hydroxyl containing monomer, 2-hydroxyethyl acrylate, resulted in an increase in the polymerization rate up to 2 times. The rate enhancement was attributed to hydrogen bonding effects and this was confirmed using the unprecedented addition of dodecanol, which also demonstrated a significant rate enhancement.
Block copolymers were also achieved using a novel difunctional nitroxide synthesized from 4-hydroxy TEMPO and 1,6-hexamethylene diisocyanate. The identity of the nitroxide was confirmed using mass spectrometry and 1H NMR. The dinitroxide was used in the polymerization of styrene and subsequently used to produce symmetric ABA triblock copolymers with t-butyl styrene using a unique two-step polymerization route. In addition, the dinitroxide demonstrated an increased tendency for decomposition due to the complex mediation equilibrium. The decomposition was studied using GPC to evaluate the decomposition effects on the polymerization.
Results of the research efforts presented herein are written as individual research reports with contributing authors and pertinent literature reviews presented at the beginning of each chapter.Ph. D.
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Alshuiref, Abubaker. "Synthesis and characterization of urethane-acrylate graft copolymers." Thesis, Link to the online version, 2006. http://hdl.handle.net/10019/491.
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Hamid, S. M. "Synthesis, aggregation behavior and polymerisation of novel amphiphilic (meth)acrylate monomers." Thesis, University of Strathclyde, 1986. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.381475.
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Poutrel, Pauline. "Réduction du motif vinyl-CF₃ : vers la synthèse catalytique énantiosélective de centres C-CF₃ et la synthèse diastéréosélective de monofluoroalcènes terminaux Copper‐catalyzed enantioselective formation of C−CF3 centers from β‐CF3‐substituted acrylates and acrylonitriles Stereoselective synthesis of terminal monofluoroalkenes from trifluoromethylated alkenes." Thesis, Normandie, 2020. http://www.theses.fr/2020NORMIR07.
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Ces dernières années, la chimie du fluor est devenue un domaine clé de recherche de par la présence croissante de l’atome du fluor dans les molécules issues de l’agrochimie, de l’industrie pharmaceutique et des matériaux. Il est alors nécessaire de développer de nouvelles méthodologies permettant la synthèse de ces molécules fluorées. Dans notre cas, il s’agit de mettre au point des procédures permettant l’obtention de synthons d’une part avec un centre stéréogène contrôlé comportant un motif trifluorométhyle, d’autre part avec un motif monofluoroalcène terminal. Dans un premier temps, nous avons développé une méthodologie pour la réduction catalytique asymétrique d’acrylates et d’acrylonitriles β-CF3 via la formation in-situ d’un hydrure de cuivre chiral. Dans un second temps, avons mis au point une méthodologie de synthèse de monofluoroalcènes terminaux par réduction au LiAlH4 d’acrylates β-CF3 et de styrènes α-CF3 di-, tri- ou tétrasubstituésIn recent years, organofluorine chemistry has become a key field of research thanks to the growing presence of the fluorine atom in molecules coming from agrochemistry, pharmaceutical industry and materials. It is therefore necessary to develop new methodologies for the synthesis of fluorinated molecules. In our case, we envisioned to develop procedures to obtain synthons with a stereogenic center bearing a trifluoromethyl group on the one hand, and synthons with a terminal monofluoroalkene motif on the other hand. We first developed a methodology for the catalytic asymmetric reduction of β-CF3 acrylates and acrylonitriles via the formation in-situ of a chiral copper hydride species. We then developed a methodology for the synthesis of terminal monofluoroalkenes by reduction of di-, tri- or tetrasubstitued β-CF3 acrylates and α-CF3 styrenes with LiAlH4
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Johnson, Harry Dale. "Synthesis, Characterization, Processing and Physical Behavior of Melt-Processible Acrylonitrile Co- and Terpolymers for Carbon Fibers: Effect of Synthetic Variables on Copolymer Synthesis." Thesis, Virginia Tech, 2006. http://hdl.handle.net/10919/32373.
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A novel photocrosslinkable and melt processible terpolymer precursor for carbon fibers has been successfully synthesized and characterized. The terpolymer was synthesized by an efficient emulsion polymerization route and has a typical composition of acrylonitrile/ methyl acrylate/acryloyl benzophenone in the molar ratio of 85/14/1. This thesis describes a systematic variation of the polymerization variables in the emulsion polymerization which may further enhance the system. In particular, the effects of chain transfer agent, initiator, and surfactant concentration on the polymer properties were studied.Master of Science
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Yu, Elsie. "Catalytic Stereoselective Olefin Metathesis for Natural Product Synthesis." Thesis, Boston College, 2018. http://hdl.handle.net/2345/bc-ir:107714.
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Thesis advisor: Amir H. HoveydaChapter 1. Efficient Z-Selective Synthesis of Allylic- and Alkenyl Boronates by Catalytic Cross-Metathesis Efficient Z-selective cross-metathesis reactions to furnish Z-(pinacolato)-allylboron and Z-(pinacolato)alkenylboron compounds through catalytic cross-metathesis are disclosed. Z-allylic boron compounds are generated by the use of catalytic amounts of a W-based monoaryloxide monopyrrolide (MAP) complex in up to 91% yield and 96:4 dr after allylation to benzaldehyde. Alkenylboron compounds are prepared in high yields and high Z selectivity in up to 93% yield and 97:3 Z:E. Cross-metathesis reactions with 1,3-dienes and aryl olefins are efficient and highly Z-selective. Combination of cross-metathesis and cross-coupling to synthesize anticancer agent combretastatin A-4 highlights the utility of this approach. Chapter 2. Synthesis of Macrocyclic and Acyclic Z-Enoates and (E,Z) or (Z,E) Dienoates by Catalytic Cross-Metathesis The first examples of kinetically controlled catalytic olefin metathesis reactions to generate Z-α,β-unsaturated macrocyclic and acyclic esters are disclosed. The synthesis of (E,Z) or (Z,E)-dienoates are also presented. Reactions promoted by 3.0–10 mol % of Mo-based monoaryloxide monopyrrolide complex proceed to completion to the desired macrocycles within 2–6 h at room temperature. Macrocycles of diverse ring sizes are formed in 79:21 to >98:2 Z:E selectivity. Pure Z isomers can be obtained after purification in up to 75% yield. Acyclic Z-α,β-unsaturated esters are prepared in the presence of acetonitrile to avoid using excess amounts of the more valuable cross-partner substrate. Spectroscopic investigations and X-ray analysis rationalize the positive effect of acetonitrile in the reaction system. Linear (Z)-enoates are generated in up to 71% yield and up to >98:2 Z:E. (E,Z)-Dienoates are generated with high Z selectivity as well. The utility of the ring-closing metathesis and cross-metathesis is highlighted by the synthesis of an (+)-aspicilin precursor and the C1–C12 fragment of biologically active natural product (–)-laulimalide. Chapter 3. Application of E-Selective Catalytic Ring-Closing Metathesis in the Total Synthesis of Dolabelides A, B, C and D Efforts towards the enantioselective synthesis of the dolabelide family of anti-cancer macrolides is presented. Development of a total synthesis incorporating a late-stage kinetically E-selective RCM is illustrated. Previous attempts to synthesize the macrolide by ring-closing metathesis (RCM) have demonstrated poor efficiency and low selectivity for the E isomer. Methodology developed in our group with acyclic trisubstituted cross-metathesis demonstrates that high selectivity can be achieved with stereodefined 1,2-disubstituted and trisubstituted olefins by the use of the proper catalyst and reaction design. Modern catalytic and stereoselective approaches towards the two main fragments of dolabelide are presented. More efficient and concise routes will be pursued to highlight the utility of the proposed disconnections and practicality of the total synthesis
Thesis (PhD) — Boston College, 2018
Submitted to: Boston College. Graduate School of Arts and Sciences
Discipline: Chemistry
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Hu, Chaohe. "Versatile biobased particles of acrylate vegetable oils : Synthesis and applications." Thesis, université Paris-Saclay, 2022. http://www.theses.fr/2022UPAST081.
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Depuis ses débuts, au début des années 1920, l'industrie des polymères dépend fortement des ressources en combustibles fossiles. Environ 4 à 8 % du pétrole, du gaz et de leurs dérivés sont aujourd'hui transformés en matériaux polymères. La plupart d'entre eux sont non recyclables et non dégradables, ce qui entraîne de graves problèmes environnementaux, préjudiciables à la faune et à l'homme. Dans ce contexte, il est nécessaire de développer des produits polymères alternatifs qui, à partir de matières premières renouvelables, présenteront le même niveau de complexité que les produits actuels issus de l'industrie pétrolière.Parmi les différentes matières premières biosourcées utilisées pour fabriquer des matériaux polymères, les huiles végétales sont prometteuses pour leur faible coût et leur dégradabilité intrinsèque, mais aussi parce que leur production est déjà optimisée pour l'industrie alimentaire. L'huile de soja époxydée acrylée (AESO) est un exemple des dérivés d'huiles végétales qui sont utilisés comme additifs plastifiants pour la formulation du PVC. Seule, l'AESO peut être facilement et rapidement polymérisée pour donner un polymère thermodurci. Cependant, en raison de sa viscosité intrinsèque élevée, la plupart des recherches sur les polymères à base d'AESO se sont concentrées jusqu'à présent sur les propriétés de masse, de revêtement ou de film de ce matériau, laissant dans l'ombre la possibilité de fabriquer des matériaux à haute valeur ajoutée.Ce travail se concentre sur la fabrication et l'application des microparticules d'AESO. Nous présentons d'abord une approche simple à travers un mélangeur vortex pour préparer les particules AESO polydispersées basées sur la photopolymérisation en émulsion. Les microparticules AESO synthétisées présentent une bonne dégradabilité dans des conditions chimiques et enzymatiques. Ensuite, nous développons un dispositif microfluidique " one pot " avec une structure de focalisation du flux pour l'émulsification et une zone serpentine pour la réticulation induite par les UV, qui peut être utilisé pour produire en continu des particules AESO monodispersées avec une taille réglable. Nous démontrons également la méthode basée sur les puces microfluidiques modifiées pour préparer les particules non sphériques, où une puce avec une jonction de focalisation d'écoulement en forme de Y est utilisée pour préparer les particules AESO en forme de croissant et une autre puce avec une double jonction de focalisation d'écoulement est utilisée pour synthétiser les particules AESO structurées en coquille de trou. De plus, des microcapsules d'AESO sont fabriquées par la puce personnalisée et elles sont disponibles pour encapsuler des solutions ou des substances aqueuses. Enfin, nous montrons la capacité des microparticules AESO à transporter les molécules organiques dans leurs réseaux réticulés et utilisons des méthodes similaires pour charger les médicaments (curcumine et ibuprofène). Le comportement de libération des médicaments dans le fluide corporel simulé peut être observé, ce qui peut constituer un support prometteur pour d'autres applications pharmaceutiquesSince its beginning, in the early 1920's, polymeric industry relies heavily on fossil fuel resources. Approximately 4%-8% oil, gas and their derivatives are nowadays transformed into polymeric materials. Most of them are non-recyclable and non-degradable, hence leading to serious environmental issues, detrimental to wildlife and humans. In this context, there is a need for the development of alternative polymeric products, which, starting from renewable commodities, will share the same level of complexity than current ones derived from oil industry.Among the various bio-sourced raw products used to make polymeric materials, vegetable oils are promising for their low cost and intrinsic degradability, but also because their production is already optimized for the food industry. Acrylated epoxidized soybean oil (AESO) is one example of the vegetable oil derivatives that are used as e.g. plastifying additives for the formulation of PVC. Alone, AESO can be readily and rapidly polymerized to give a thermoset polymer. However, as a consequence of its high intrinsic viscosity, most of the research on AESO-based polymer so far is only focused on the bulk, coating or film properties of this material, leaving the possibility to fabricate high added value materials a blind spot.Herein, this work focuses on the fabrication and application of the AESO microparticles. We first present a simple approach through a vortex mixer to prepare the polydispersed AESO particles based on the emulsion photopolymerization. The synthesized AESO microparticles present a good degradability in the chemical and enzymatic conditions. Then, we develop a “one pot” microfluidic device with a flow-focusing structure for emulsification and the serpentine zone for UV-induced reticulation, which can be used to continuously product the monodispersed AESO particles with a tunable size. We also demonstrate the method base on the modified microfluidic chips to prepare the non-spherical particles, where a chip with Y-shape flow-focusing junction is used to prepare the crescent-shaped AESO particles and another chip with a double flow-focusing junction is utilized to synthesize the hole-shell structured AESO particles. In addition, AESO microcapsules are fabricated by the customized chip, and they are available to encapsulate the aqueous solutions or substances. Finally, we show the ability of AESO microparticles to carry the organic molecules into their crosslinked networks and use the similar methods to load the drugs (curcumin and ibuprofen). The release behavior of drugs in simulated body fluid can be observed, which may be act as a promising drug carrier for further pharmacy applications
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Zeytin, Cigdem. "Synthesis And Characterization Of Epoxy-acrylate Vinylester Resin And Network Structure." Phd thesis, METU, 2008. http://etd.lib.metu.edu.tr/upload/3/12610115/index.pdf.
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Vinylesters are termosets resins that have reactive double bond at the chain ends. They are produced by the reaction of various epoxies and acrylic acids by step growth polymerization. Vinylester chains are oligomers with molecular weight from 600 to 1200 g/mol. The resin viscosity is very hightherefore, diluent is used for easy application. The generally used diluent is styrene with, reactive double bonds to form a crosslink between the chains. The diluted resin viscosities are between 200 &
#8211
2000 cps. Peroxide initiators are used for network formation. The mechanical properties of vinylester resin are enhanced with reinforcements such as glass fiber, carbon fiber, Kevlar or nanoparticules to make composites. Various molecular weights of vinylester resins were synthesized and the samples were prepared with different styrene contents. The effects of the styrene content, temperature and molecular weight on the viscosity were measured and examined. The main effects were determined as styrene content and temperature, while the effect of molecular weight is negligible. The resins were characterized with IR and NMR spectroscopy. The molecular weights were determined by theoretical calculations, titration and H-NMR spectroscopy. Peroxide initiators were used to cure the resins with the cobalt complex accelerator. The resins were post-cured at different temperatures. The completion of the curing was monitored by the disappearance of the carbon-carbon double bonds of methacrylate (943 cm-1) and styrene (910 cm-1), by FT-IR spectrum. The effects of styrene content, post-cure conditions, and molecular weight on the mechanical properties were discussed. The glass transition temperatures were determined by DSC and DMA. The crosslink densities and rheological properties were determined by creep test. The important properties of vinylester resins, which are modulus, tensile and flexural strength, shrinkage, water absorption, glass transition temperature, HDT values and impact strength were investigated.
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Bradley, Grant. "Hexaarylbisimidazoles as initiators of acrylate polymerisation : some new synthesis and application." Thesis, University of Kent, 1997. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.360967.
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MacDonald, Iain I. "Synthesis, structural and adhesive evaluation of novel graft meth(acrylate) copolymers." Thesis, University of Strathclyde, 2011. http://oleg.lib.strath.ac.uk:80/R/?func=dbin-jump-full&object_id=15334.
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Piunova, Victoria A. "Photopolymerizable “Roundup” Synthesis, Herbicidal Activity and Coating Formulation." Bowling Green State University / OhioLINK, 2006. http://rave.ohiolink.edu/etdc/view?acc_num=bgsu1151340117.
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Auty, Samuel. "Utilising novel thiol-acrylate click reactions to synthesise controlled branched polymer emulsifiers." Thesis, University of Liverpool, 2014. http://livrepository.liverpool.ac.uk/2007707/.
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The formation of multi-functional thiol materials for “click” reactions in synthetic chemistry has been significantly under-represented due to added practices that are typically required when working with sulfur-containing compounds. An efficient and facile approach to approach to introducing multiple masked thiols at the surface of polyester dendritic materials is presented, avoiding these difficulties, by utilising a xanthate protecting group. One-pot xanthate deprotection and thiol-acrylate Michael additions from the xanthate-functional dendrimers (generation zero to two) has been accomplished for the first time, using three different acrylate substrates of varying chemistry. The dendrimers were fully characterised by 1H and 13C NMR, SEC and either electrospray or MALDI-TOF mass spectrometry, depending upon the generation and nature of the end groups. In a similar fashion, this one-pot methodology was extended to prepare twenty different surface functional LDHs via the use of xanthate functional ATRP dendritic macroinitiators (generation one to four) and six different acrylate monomers. Model reactions and kinetics studies showed that the presence of xanthates within the initiator structure did not complicate the ATRP of tBuMA. The LDHs were fully characterised by 1H NMR and SEC. In the final study, employing one-pot xanthate deprotection and thiol-acrylate Michael addition, four dendritic ATRP macroinitiators with hydrophobic and pH responsive peripheral functionalities were prepared. Polymeric surfactants comprised of LDHs and HPDs were synthesised, varying in end group composition using different dendritic macroinitiators, and through the use of mixed initiating system, using a non-dendritic component. O/w emulsions stabilised by surfactants comprised of linear polymers, LDHs, or mixed linear polymers/LDHs architectures showed coalescence over a long term stability study under neutral and acid conditions. In contrast, o/w emulsions stabilised by surfactants comprised of branched polymers, HPDs, or mixed branched polymer/HPDs architectures showed no coalescence over a long term stability study under neutral and acid conditions. Further dilution and thermal studies to probe emulsion systems stabilised via branched surfactant architectures resulted in emulsion breakdown.
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Chai, Qinyuan. "Synthesis and Characterization of Ionically Crosslinked Networks." University of Akron / OhioLINK, 2013. http://rave.ohiolink.edu/etdc/view?acc_num=akron1367939178.
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Cheshmehkani, Ameneh. "Design and synthesis of molecular resists for high resolution patterning performance." Thesis, Georgia Institute of Technology, 2013. http://hdl.handle.net/1853/50286.
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In this thesis, different approaches in synthesizing molecular resist are examined, and structure-property relations for the molecular resist properties are studied. This allows for design of resists that could be studied further as either negative or positive tone resists in photolithography. A series of compounds having different number of acrylate moiety, and different backbones were investigated for photoresist application. Thermal curing of acrylate compounds in organic solvent was also examined. Film shrinkage, as well as auto-polymerization was observed for these compounds that make them unsuitable as photoresist material. Furthermore, calix[4]resorcinarenes (C4MR) was chosen as backbone, and the functional groups was selected as oxetane and epoxy. Full functionalized C4MR compounds with oxetane, epoxy and allyl were synthesized. Variable-temperature NMR of C4MR-8Allyl was studied in order to get a better understanding of the structure’s conformers. Energy barrier of exchange (ΔG#) was determined from coalescence temperatures, and was 57.4 KJ/mol for aromatic and vinyl hydrogens and 62.1 KJ/mol for allylic hydrogens.
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Keskin, Selda. "Synthesis And Characterization Of Copolymers Of Diisocyanates And Dialcohol." Phd thesis, METU, 2008. http://etd.lib.metu.edu.tr/upload/3/12609995/index.pdf.
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This study was aimed to synthesize low molecular weight hydroxyl terminated polyurethane acrylate polymers that can be used in biomedical applications. Acrylate end capping via inter-esterification reaction was successfully achieved with the methacryloyl chloride addition to the hydroxyl ends of the polyurethane at low temperatures. Isocyanate terminated polyurethane acrylates were also synthesized for the sake of comparison. TDI, HDI and MDI were used as diisocyanates for urethane synthesis and they were end capped with MMA and HEMA. Nature of the monomers used had an effect on thermal, morphological, and rheological properties that were interpreted in terms of the level of hydrogen bonding and degree of phase separation. Synthesized polymers were characterized by NMR, FTIR-ATR, DSC, TGA, GPC, Mass Spectroscopy, SEM and rheometry.
In the literature, polyurethane acrylate polymers have been synthesized from the isocyanate terminated polyurethanes in which the urethane chains were ended with isocyanate groups. However, the toxicity of the isocyanate groups limited their biomedical applications especially in prosthetic dentistry as a soft lining material. Therefore, it is inevitable to explore the cytotoxicity of polyurethane acrylate polymers. For this purpose, silver nanoparticles that have an average particle size of 40 nm, were incorporated to the synthesized polymers. This addition, which intends to improve the degree of cytotoxicity, was successful to a certain extent.
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Wang, Yi. "The Synthesis and Characterization of Amphiphilic Poly(Ethylene Oxide)-Block-Poly(Octadecyl Acrylate) Block Copolymers." University of Akron / OhioLINK, 2014. http://rave.ohiolink.edu/etdc/view?acc_num=akron1399491109.
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GOMES, FREIRE-SCHANZ MARIA TELMA. "Synthese et caracterisation de nouveaux (co) polymeres a base de monomeres carbonates de vinyle et acrylates." Université Louis Pasteur (Strasbourg) (1971-2008), 1989. http://www.theses.fr/1989STR13132.
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Divers monomeres carbonate de vinyle aromatiques et aliphatiques ont ete polymerises en masse a 35#oc. L'amorcage resulte de la decomposition du percarbonate de bis-(4 tertiobutylcyclohexyle), ce qui a permis d'obtenir des polymeres de masses moleculaires elevees. L'effet du radical substituant sur les proprietes physico-chimiques des polymeres a ete etudie. Certains de ces monomeres ont ensuite ete copolymerises avec le styrene et le methacrylate de methyle en solution dans le dichloromethane a 70#oc, en presence d'azobisisobutyronitrile. Les rapports de reactivite r#1 et r#2 ont ete determines par la methode de kelen-tudos. Une nouvelle serie de monomeres acryliques u-substitues a ete (co)polymerisee en emulsion avec le styrene et l'acrylate de methyle a 70#oc, en presence de persulfate de potassium. L'evolution cinetique des (co)polymerisations a ete etudiee en fonction de la nature et de la concentration en monomere acrylique, et de la quantite d'amorceur et d'emulsifiant. La composition et les proprietes physico-chimiques des (co)-polymeres resultants, ainsi que les proprietes coloidales des latex, ont ete etudiees par irtf, #1hrmn, gpc, dsc, ddl, tensiometrie et viscosimetrie
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Tichagwa, Lilian M. "Synthesis of acrylate-based polymeric and polymerisable surfactants and their application in the emulsion polymerisation of styrene." Thesis, Stellenbosch : University of Stellenbosch, 2006. http://hdl.handle.net/10019.1/1185.
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Thesis (PhD (Chemistry and Polymer Science))--University of Stellenbosch, 2006.The study described in this dissertation examines the synthesis of mainly acrylate-based surfactants and their subsequent use as emulsifiers/stabilisers in the emulsion polymerisation of styrene. Some acrylamide-based surfactants were also studied, for comparison purposes only. Two major types of surfactants, polymerisable (surfactant monomers or surfmers) and polymeric, were synthesised, characterised and used in emulsion polymerisation reactions. The prepared polymerisable surfactants, 12-acryloyloxydodecanoic acid (12-ADA) and 11-acrylamidoundecanoic acid (11-AAUA), and their sodium salts, had reactive acryloyl functionalities.
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Cox-Nowak, Kayleigh. "Synthesis and cell adhesion studies of linear and hyperbranched poly(butyl methacrylate) and poly(t-butyl acrylate)." Thesis, University of Sheffield, 2013. http://etheses.whiterose.ac.uk/4819/.
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A library of polymers/oligomers with three different architectures was synthesised. Short chain, linear oligomers were produced by performing oxidative cleavage on a poly(butyl methacrylate-co-butadiene) polymer. Although butadiene is a gaseous monomer, it was found that careful control over the reaction conditions led to successful copolymerisation in an unpressurised reactor. Hyperbranched polymers of n-butyl methacrylate and t-butyl acrylate were synthesised by RAFT polymerisation with 4-vinylbenzyl-pyrrolecarbodithioate (CTA1) and 4-vinylbenzyl dithiobenzoate (CTA2). A variety of analytical techniques, such as elemental analysis and NMR, were used to characterise the polymers and confirm the hyperbranched structure. Some variation in monomer conversion and CTA uptake was seen under different polymerisation conditions. After synthesis and characterisation, it was found that the polymer end groups could be modified through work up with diamine or 4.4‘-azobiscyanovaleric acid. Linear oligomers of butyl methacrylate were functionalised with amines whilst hyperbranched polymers were given acid functional end groups. FT-IR and elemental analysis were used to monitor the success of the end group reactions. As the polymers could be applied as films, they were assessed as cell culture substrates using Human dermal fibroblasts (HDF) and Human renal epithelial cells (HREp). A linear butyl methacrylate-co-4-vinyl benzoic acid copolymer was also assessed in comparison to the hyperbranched structures. It was observed that the two cell types had different responses to each of the polymers. Fibroblast cells showed better rates of adhesion and proliferation on acid-functionalised polymers, whilst epithelial cells performed best on the aminefunctionalised moieties. This work provides useful information for the synthesis and preparation of new biomaterials. It has been found that polymer functionality must be considered when compatibility with a specific cell type is desired, and polymers with the potential to be incorporated into future biomaterials are highlighted.
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Wu, Tianyu. "Synthesis and Characterization of Zwitterion-Containing Acrylic (Block) Copolymers for Emerging Electroactive and Biomedical Applications." Diss., Virginia Tech, 2012. http://hdl.handle.net/10919/39332.
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Conventional free radical polymerization of n-butyl acrylate with 3-[[2-(methacryloyloxy)ethyl](dimethyl)-ammonio]-1-propanesulfonate (SBMA) and 2-[butyl(dimethyl)amino]ethyl methacrylate methanesulfonate (BDMAEMA MS), respectively, yielded zwitterionomers and cationomers of comparable chemical structures. Differential scanning calorimetry (DSC), small-angle X-ray scattering (SAXS), and atomic force microscopy (AFM) revealed that zwitterionomers promoted more well-defined microphase-separation than cationic analogs. Dynamic mechanical analyses (DMA) of the copolymers showed a rubbery plateau region due to physical crosslinks between charges for zwitterionomers only. We attributed improved microphase-separation and superior elastomeric performance of the zwitterionomers to stronger association between covalently tethered charged pairs.
Zwitterionomer / ionic liquid binary compositions of poly(nBA-co-SBMA) and 1-ethyl-3-methylimidazolium ethylsulfate (EMIm ES) were prepared using both the 'swelling– and the –cast with– methods. Dynamic mechanical analysis revealed that the 'swollen– membranes maintained their thermomechanical performance with up to 18 wt% EMIm ES incorporation, while that of the –cast with– membranes decreased gradually as the ionic liquid concentration in the composite membranes increased. Small-angle X-ray scattering results indicated that the 'swollen– and the –cast with– membranes have different morphologies, with the ionic liquid distributed more evenly inside the –cast with– membranes. Impedance spectroscopy results showed that the –cast with– membranes had better ionic conductivity than the 'swollen– membrane at high ionic liquid concentration, in agreement with our proposed model. The results indicated that the different processing methods had a significant impact on thermomechanical properties, ionic conductivities, as well as morphologies of the zwitterionomer / ionic liquid binary compositions.
Reversible addition-fragmentation chain transfer polymerization (RAFT) strategy afforded the synthesis of well-defined poly(sty-b-nBA-b-sty). 2-(Dimethylamino)ethyl acrylate (DMAEA), a tertiary amine-containing acrylic monomer, exhibited radical chain transfer tendency toward itself, which is undesirable in controlled radical polymerization processes. We employed a higher [RAFT] : [Initiator] ratio of 20 : 1 to minimize the impact of the chain transfer reactions and yielded high molecular weight poly[sty-b-(nBA-co-DMAEA)-b-sty] with relatively narrow PDIs. The presence of the tertiary amine functionality, as well as their quaternized derivatives, in the central blocks of the triblock copolymers afforded them tunable polarity toward polar guest molecules, such as ionic liquids. Gravimetric measurements determined the swelling capacity of the triblock copolymers for EMIm TfO, an ionic liquid. DSC and DMA results revealed the impact of the ionic liquid on the thermal and thermomechanical properties of the triblock copolymers, respectively. Composite membranes of DMAEA-derived triblock copolymers and EMIm TfO exhibited desirable plateau moduli of ~ 100 MPa, and were hence fabricated into electromechanical transducers.
RAFT synthesized poly(sty-b-nBA-b-sty) triblock copolymer phase separates into long-range ordered morphologies in the solid state due to the incompatibility between the poly(nBA) phases and the poly(sty) phases. The incorporation of DMAEA into the central acrylic blocks enabled subsequent quaternization of the tertiary amines into sulfobetaine functionalities. Both DSC and DMA results suggested that the electrostatic interactions in the low Tg central blocks of poly(sty-b-nBA-b-sty) enhanced block copolymer phase separation. SAXS results indicated that the presence of the sulfobetaine functionalities in acrylate phases increased electron density differences between the phases, and led to better defined scattering profiles. TEM results confirmed that the block copolymers of designed molecular weights exhibited lamellar morphologies, and the lamellar spacing increased with the amount of electrostatic interactions for the zwitterionic triblock copolymers.
Acrylic radicals are more susceptible to radical chain transfer than their styrenic and methacrylic counterparts. Controlled radical polymerization processes (e.g. RAFT, ATRP and NMP) mediate the reactivity of the acrylic radical and enable the synthesis of well-defined linear poly(alkyl acrylate)s. However, functional groups such as tertiary amine and imidazole on acrylic monomers interfere with the controlled radical polymerization of functional acrylates. Model CFR and RAFT polymerization of nBA in the presence of triethylamine and N-methyl imidazole revealed the interference of the functional group on the polymerization of acrylate. Various RAFT agents, RAFT agent to initiator ratios, degree of polymerization and monomer feed concentrations were screened with an imidazole-containing acrylate for optimized RAFT polymerization conditions. The results suggest that the controlled radical polymerization of functional acrylates, such as 2-(dimethylamino)ethyl acrylate and 4-((3-(1H-imidazole-1-yl)propanoyl)oxy)-butyl acrylate (ImPBA), remained challenging.Ph. D.
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Beck, Susan Ashley. "Copolymerizing Acrylonitrile and Methyl Acrylate by RAFT for Melt Processing Applications: A Synthetic Investigation of the Effects of Chain Transfer Agent, Initiator, Temperature, and Solvent." Thesis, Virginia Tech, 2014. http://hdl.handle.net/10919/49104.
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Statistical copolymers of acrylonitrile (AN) and methyl acrylate (MA) were successfully prepared and characterized using reversible addition-fragmentation chain transfer (RAFT) copolymerization. A typical copolymer was charged with 15 wt. % MA content. This thesis describes a systematic variation of the RAFT copolymerization variables to optimize this system. In particular, the effects of chain transfer agent, initiator, temperature, and solvent on the copolymer properties were studied.Master of Science
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Appelt, Mathias. "Synthese von Co-, Stern- und Pfropfpolymeren aus Styrol und Acrylsäurederivaten durch N-Oxyl kontrollierte radikalische Polymerisation." [S.l. : s.n.], 2003. http://deposit.ddb.de/cgi-bin/dokserv?idn=968459447.
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Pisipati, Padmapriya. "Synthesis and Characterization of Solution and Melt Processible Poly(acrylonitrile-co-methylacrylate) statistical copolymers." Diss., Virginia Tech, 2015. http://hdl.handle.net/10919/73150.
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Polyacrylonitrile (PAN) and its copolymers are used in a wide variety of applications ranging from textiles to purification membranes, packaging material and carbon fiber precursors. High performance polyacrylonitrile copolymer fiber is the most dominant precursor for carbon fibers. Synthesis of very high molecular weight poly(acrylonitrile-co-methyl acrylate) copolymers with weight average molecular weights of at least 1.7 million g/mole were synthesized on a laboratory scale using low temperature, emulsion copolymerization in a closed pressure reactor. Single filaments were spun via hybrid dry-jet gel solution spinning. These very high molecular weight copolymers produced precursor fibers with tensile strengths averaging 954 MPa with an elastic modulus of 15.9 GPa (N = 296). The small filament diameters were approximately 5 'm. Results indicated that the low filament diameter that was achieved with a high draw ratio, combined with the hybrid dry-jet gel spinning process lead to an exponential enhancement of the tensile properties of these fibers.
Carbon fibers for polymer matrix composites are currently derived from polyacrylonitrile copolymer fiber precursors where solution spinning accounts for ~40 % of the total fiber production cost. To expand carbon fiber applications into the automotive industry, the cost of the carbon fiber needs to be reduced from $8 to ~$3-5. In order to develop an alternative melt processing route several benign plasticizers have been investigated. A low temperature, persulfate-metabisulfite initiated emulsion copolymerization was developed to synthesize poly(acrylonitrile-co-methyl acrylate) copolymers with acrylonitrile contents between 91-96 wt% with a molecular weight range of 100-200 kg/mol. This method was designed for a potential industrial scale up. Furthermore, water was investigated as a potential melting point depressant for these copolymers. Twenty-five wt% water lead to a decrease in the Tm of a 93/7 wt/wt % poly(acrylonitrile-co-methyl acrylate) of Mw = 200 kg/mol to 160 0C as measured via DSC.
Glycerin, ethylene glycol and glycerin/water combinations were investigated as potential plasticizers for high molecular weight (~200,000 g/mol), high acrylonitrile (93-96 mole:mole %) content poly(acrylonitrile–co-methyl acrylate) statistical copolymers. Pure glycerin (25 wt %) induced crystallization followed by a reduced "Tm" of about 213 °C via DSC. However this composition did not melt process well. A lower MW (~35 kg/mol) copolymer did extrude with no apparent degradation. Our hypothesis is that the hydroxyl groups in glycerin (or water) disrupt the strong dipole-dipole interactions between the chains enabling the copolymer endothermic transition (Tm) to be reduced and enable melting before the onset of degradation. Additionally high molecular weight (Mw = 200-230 kg/mol) poly(acrylonitrile–co-methyl acrylate) copolymers with lower acrylonitrile content (82-85 wt %) were synthesized via emulsion copolymerization and successfully melt pressed. These materials will be further investigated for their utility in packaging applications.Ph. D.
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Huzyak, Paige M. "Synthesis and Characterization of Organic-Inorganic Hybrid Materials for Thermoelectric Devices." TopSCHOLAR®, 2016. http://digitalcommons.wku.edu/theses/1600.
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The development of organic-inorganic hybrid materials is of great interest in thermoelectrics for its potential to combine the desirable characteristics of both classes of materials. Thermoelectric materials must combine low thermal conductivity with high electrical conductivity, but in most materials, thermal and electrical conductivity are closely related and positively correlated. By combining the low thermal conductivity, flexibility, facile processing, and low cost of organic components with the high electrical conductivity and stability of inorganic components, materials with beneficial thermoelectric properties may be realized.
Here, we describe the synthesis and characterization of anthracene-containing organic-inorganic hybrid materials for thermoelectric purposes. Specifically, POSS-ANT was synthesized when aminopropylisobutyl-POSS was functionalized with a single anthracene unit via DCC-mediated amide formation. Acrylate-POSS was functionalized with multiple anthracene units in a Heck coupling reaction to synthesize System 1. System 2 was developed through a two-step synthetic process. In the first reaction, (3- acryloxypropyl)methyl dimethyoxy silane was functionalized with anthracene at the 9- position through a Heck coupling reaction. The second reaction was a base-catalyzed solgel process to form polymeric nanoparticles. Finally, System 3 was synthesized through a similar process to System 2, though polymers formed in the initial step. The System 3 precursor was to be developed through a potassium carbonate-catalyzed ether synthesis
from 3-(bromopropyl)trimethoxysilane and 9-anthracene methanol, followed by a basecatalyzed sol-gel process to form nanoparticles. The precursor was never isolated because of premature polymerization during the precursor synthesis step, and polymeric nanoparticles were obtained for System 3 during the sol-gel process. These materials were characterized by TEM to reveal the nanostructures that formed upon evaporation from solution. Future work will focus on the characterization of thermoelectric parameters and incorporation into thermoelectric devices.
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Bui, Nhat Thi Hong. "Polyhydroxyl and Polyphosphorylcholine functionalized Silica for Hydrophilic interaction liquid Chromatography- Synthesis, characterization and application." Doctoral thesis, Umeå universitet, Kemiska institutionen, 2012. http://urn.kb.se/resolve?urn=urn:nbn:se:umu:diva-60600.
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This thesis focuses on the development of new stationary phases for use in hydrophilic interaction liquid chromatography using TRIS-based and phosphorylcholine typed monomers and porous silica particles as starting substrates. In this thesis, several ways of polymerizing highly hydrophilic monomers onto pore surfaces of silica supports are described, based on several “grafting from” schemes. “Controlled/living” radical polymerizations including atom transfer radical polymerization (ATRP) and iniferter-mediated polymerization in conjunction with conventional free radical polymerization are demonstrated to be successful tools for grafting different hydrophilic monomers (polyhydroxyl and phosphorylcholine [meth]acrylamide/acrylates) onto the silica surfaces. Reaction solvents are proven to play an essential role to achieve efficient graft polymerization of activated silica surfaces with these amphiphilic vinylic monomers, which is difficult because of their restricted access to the activated surface in solvents that can be used because of solubility constraints. Two tentacle TRIS-based polymer grafted silica, namely TRIS-WAX – TRIS functionality bonded to silica via a C–N–C imine bond and TRIS-Amide – TRIS bonded to silica via an amide bond, prove to be useful as stationary phases for hydrophilic interaction chromatography (HILIC).The TRIS-WAX exhibits a mixed mode hydrophilic partitioning and weak anion exchange (HILIC/WAX) retention mechanism while retention by hydrophilic partitioning is the dominant mechanism on the neutral TRIS-Amide phase which lacks weak anion exchange (WAX) properties. Interestingly, both these phases have selectivities that are radically different from most commercial HILIC stationary phases. Finally, a method is demonstrated for synthesizing a stratified (graft-copolymerized) silica material based on N,N′-methylenebisacrylamide and 2-methacryloyloxyethyl phosphorylcholine (MPC) using a “controlled/living” photoiniferter-mediated polymerization from the N,N-diethyldithiocarbamate iniferter moiety immobilized silica surfaces. This polymerization method proves to be successful for graft-blockcopolymerization of different highly hydrophilic monomers onto the activated surfaces of porous silica. In this way, silica surfaces are grafted with a cross-linked amide-based hydrogel, on top of which a tentacle zwitterionic phosphorylcholine-typed layer is synthesized. The resulted material proves to be useful for HILIC separations and possesses different selectivity for the tested organic acids compared to that of commercial ZIC-cHILIC stationary phase.
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EL, ALAMI NAJAT. "Isolement et reactivite du derive zincique de (bromomethyl-2) acrylate d'ethyle : synthese de methylene-3 pyrrolidinone-3 potentiellement antineoplasique." Nantes, 1987. http://www.theses.fr/1987NANT2016.
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Reaction de l'organozinicique allylique prepare, avec divers electrophiles conduisant a des methylene-3 perhydrofurannones-2 et -pyrrolidones-2. Etude de l'activite de ces composes sur la leucamie p388
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Nordell, Patricia. "Aluminium oxide - poly(ethylene-co-butylacrylate) nanocomposites : synthesis, structure, transport properties and long-term performance." Licentiate thesis, KTH, Polymera material, 2011. http://urn.kb.se/resolve?urn=urn:nbn:se:kth:diva-29270.
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Polymer nanocomposites are promising materials for dielectrical use in high voltage applications and insulations. This work presents a study of nanocomposites based on poly(ethylene-co-butyl acrylate) with two different comonomer compositions and two different aluminium oxide nanoparticles. The nanoparticles were either untreated, or surface-treated with two different silanes, aminopropyl triethoxy silane and octyltriethoxy silane. The best level of dispersion was found for the polymer with 13 wt. % of butyl acrylate (EBA-13) whereas the low melt viscosity of the polymer with 28 wt. % of butyl acrylate (EBA-28) resulted in insufficient mixing with uneven dispersion as a result. Octyltriethoxy silane-treated particles were best dispersed in the polymer. The nanoparticles acted as nucleation agents in EBA-28, increasing the crystallization temperature by several degrees. Studies of the water uptake in the nanocomposite materials showed the effect of the enormous interfacial surfaces and great number of polar groups present on the nanoparticle surfaces. For the well-dispersed nanomaterials, the water sorption data could be modeled by a single Fickian equation, whereas materials that contained a sizeable fraction of large nanoparticle agglomerates showed a two stage sorption process, first a fast process associated with the saturation of the polymer phase and second, a slow diffusion process due to water sorption of large particle agglomerates. The long-term performance and interaction between the nanoparticles and the phenolic antioxidant (Irganox 1010) was investigated by differential scanning calorimetry in order to assess the oxidation induction time (OIT); the latter being proportional to the concentration of efficient antioxidant. It was found that the stabilizer was adsorbed to the untreated Al2O3 nanoparticles, resulting in a significant reduction in OIT. However, silanization of the nanoparticles resulted in an increase in OIT, compared to the materials containing untreated particles. Furthermore, it was shown that the stabilizer was not irreversibly adsorbed to the particles, allowing a gradual release of stabilizer with ageing time.Polymera nanokompositer är lovande material för användning som dielektriskt material inom högspänningsområdet. I detta arbete studeras nanokompositer framställda av två olika sampolymerer av eten och butylakrylat (EBA-13 med 13 vikt% butylakrylat samt EBA-28 med 28 vikt% och två olika typer av nanopartiklar av Al2O3. Nanopartiklarna användes antingen som obehandlade eller efter silanisering med aminopropyltrietoxysilan- eller oktyltrietoxysilan. Den bästa partikeldispergeringen observerades för de material som baserats på EBA-13 medan den låga smältviskositeten hos EBA-28 resulterade i låga skjuvkrafter under kompounderingen och en observerat ojämn dispergering och förekomst av mikrometerstora agglomerat. Partiklar som silaniserats med oktyltrietoxysilan var lättast att dispergera. Nanopartiklarna fungerade som kärnbildare i EBA-28 vilket medförde en höjning av kristallisationstemperaturen. Vattensorptionsstudier demonstrerade dels effekten av den stora specifika gränsytan mellan partikel och matris och dels av förekomst av polära grupper lokaliserade till nämnda gränsyta. Kompositer med väldispergerade partiklar uppvisade en enkel Ficksk sorptionsprocess medan de material som innehöll en betydande mängd stora agglomerat påvisade en tvådelad process. Den första processen var kopplad till mättningen av polymermatrisen och den andra kunde länkas till vattenupptaget i de stora agglomeraten. Vidare undersöktes långtidsegenskaperna hos nanokompositerna, samt om det fanns någon växelverkan mellan nanopartiklar och en fenolbaserade antioxidant (Irganox 1010). DSC användes för att bestämma induktionstiden för oxidation (OIT) vilket är ett mått på koncentrationen av aktiv fenolisk antioxidant. Det framgick det att Irganox 1010 adsorberades på nanopartiklarna, vilket ledde till en minskning av OIT. Det framgick även att de material som innehöll silaniserade nanopartiklar hade högre OIT jämfört material med obehandlade partiklar. Antioxidanten var däremot inte irreversibelt bunden till nanopartiklarna, utan frigjordes från deras ytor och blev aktiv under åldringen.
QC 20110128
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Zheng, Yanling. "Polymeres zwitterioniques : synthese, proprietes en solution et en masse." Université Louis Pasteur (Strasbourg) (1971-2008), 1987. http://www.theses.fr/1987STR13092.
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Copolymeres a base d'acrylate d'ethyle et porteurs de groupes lateraux zwitterionique de structure variee, soit par voie radicalaire soit par quaternarisation des precurseurs contenant une amine tertiaire. Complexation d'anion polarisable sur un homopolymere du type sulfopropylbetaine
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García, Romero Iván. "Kombinatorische Methoden zur Bestimmung der chemischen Heterogenität und der Phasenseparation von statistischen Copolymeren." [S.l.] : [s.n.], 2006. http://elib.tu-darmstadt.de/diss/000754.
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Gérard, David. "Etude de la réaction Carbamate / Aldéhyde et son application vers de nouveaux matériaux thermodurcissables." Thesis, Lyon, 2020. http://www.theses.fr/2020LYSEI105.
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La grande majorité des systèmes réticulant actuellement mis en jeu dans la synthèse de matériaux thermodurcissables nécessitent l'utilisation de composés souvent dangereux pour l'environnement comme pour les opérateurs. Les polyuréthanes, particulièrement importants car utilisés dans de nombreuses applications, ne font pas exception à cette règle. En effet, ces polymères sont classiquement obtenus par polyaddition entre un polyol et un polyisocyanate, ce dernier étant issu de dérivés du phosgène très toxiques. Le développement d'alternatives plus sûres et durables présente ainsi un intérêt particulièrement important pour les équipes de recherche tant académiques qu'industrielles. Le but de ce projet est d'explorer une nouvelle alternative pour la synthèse de matériaux polyuréthanes réticulés via la réaction entre des fonctions carbamate primaires et aldéhydes. Bien que connue depuis le 19e siècle, cette réaction n'a été utilisée pour obtenir des matériaux thermodurcissables que depuis très récemment, et ce sans jamais utiliser de composés biosourcés. Cette étude débute ainsi par la compréhension de la réaction carbamate / aldéhyde en elle-même à travers l'étude de différentes réactions modèles monofonctionnelles afin de valider la faisabilité de notre stratégie. Notre proposition d'un mécanisme réactionnel vient compléter cette étude fondamentale afin de comprendre au mieux les paramètres clés de cette réaction. Nous nous sommes par la suite intéressé à des systèmes polyfonctionnels afin d'obtenir des polyuréthanes linéaires puis tridimensionnels par cette réaction, mettant en jeu des composés biosourcés, jusqu'à l'élaboration et la caractérisation des polymères obtenus. Ce travail constitue ainsi un socle sur lequel des études suivantes peuvent s'appuyer pour élaborer de nouveaux matériaux polyuréthane thermodurcissables biosourcés sans isocyanate ni phosgèneThe vast majority of the crosslinking systems currently involved in the synthesis of thermosetting resins require the use of hazardous components for the environment as well as for the operators. Polyurethanes (PU), which are among the most important polymer materials thanks to their versatile properties, are not an exception to this issue. Polyurethanes are indeed classically obtained by polyaddition between a polyol and a polyisocyanate, the synthesis of the latter involving the use of highly toxic phosgene derivatives. The development of safer and more eco-friendly alternatives to those already existing crosslinking systems are thus of particular interest for both academic and industrial research teams. The aim of this project is to explore a new alternative for the synthesis of crosslinked polyurethanes via the reaction between primary carbamate and aldehyde functions. Although being known since the 19th century, this reaction hasn’t been used to make crosslinked polymers until very recently, without exploring biobased alternatives. This work starts with the comprehensive study of the carbamate / aldehyde reaction through model reactions in order to validate the feasibility of this new route. A proposed mechanism completes this fundamental study aiming to understand the key parameters of this reaction. In the next part of our work, we applied this knowledge to multifunctionnal systems, in order to obtain linear PU oligomers and PU networks using biobased precursors
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Tobing, Singa D. "Synthesis and structure property studies in acrylic pressure sensitive adhesives /." Diss., 1999. http://gateway.proquest.com/openurl?url_ver=Z39.88-2004&rft_val_fmt=info:ofi/fmt:kev:mtx:dissertation&res_dat=xri:pqdiss&rft_dat=xri:pqdiss:9955179.
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Chen, Wei-Chih, and 陳威志. "Synthesis and blue-light photopolymerization of branched polyurethane acrylates." Thesis, 2018. http://ndltd.ncl.edu.tw/handle/m6mqnt.
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碩士國立臺北科技大學
化學工程與生物科技系生化與生醫工程碩士班
106
Hyperbranched polyurethane acrylates (HBPUAs) were prepared via one-pot step-wise polymerization of A2/B3/BR monomers. The weight-average molecular weight of HBPUAs were approximately 1900 to 11000 g/mol. The exothermic reaction heat during blue-light photoinduced polymerization was reduced to 233 J/g with addition of the 30% of HBPUA into triethylene glycol dimethacrylate (TEGDMA) from 304 J/g of that without HBPUA. With addition of the HBPUA, the volumetric shrinkage during photopolymerization can be decreased to 7.8 % from 12.4 %. The prepared HBOUA can be as a bio-medical material, such as blue-light curable bio-adhesive.
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HUANG, PO-HAN, and 黃柏翰. "Synthesis and Properties of Nanocomposites , Copolymers and Particle Toughened PMMA Based on Novel Acrylates." Thesis, 2014. http://ndltd.ncl.edu.tw/handle/n4687j.
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碩士義守大學
生物技術與化學工程研究所
102
This research includes three major parts. The first part of the research is to copolymerize methyl methacrylate with three different monomers, which are dipropylene glycol mono-methyl ether acrylate(DOBA), propylene glycol mono-methyl ether acrylate(OBA1) and its isomers, OBA2, through the method of solution polymerization with different proportions, aollowing by the investigation of the thermal stability and the optical properties of the copolymers. The results turn out that compared with PMMA, the copolymers have an enhancement in thermal stability and better potentiality in toughness enhancement. The second part of the research is to prepare nanocomposites, POBA1/clay, POBA2/clay and PDOBA/clay. We added different proportions of modified clay into monomers of OBA1, OBA2 and DOBA. Then, we synthesized nanocomposites, POBA1/clay, POBA2/clay and PDOBA/clay by miniemulsion polymerization, and conduct investigation of their structure, thermal stability. The results show that the nanocomposites we made are intercalated nanocomposites with partially-exfoliated structure, which have a great improvement in their thermal stability. All in all, PMMA has the best optical property of all plastics. It not only excels in weatherability, but also has a wide range of application. However, PMMA is brittle, which makes its impact resistance unideal. Therefore, the third part of the research is to produce particle toughened PMMA to improve its impact resistance. In the experiments, we prepare particles of POBA1, POBA2 and PDOBA by emulsifier-free emulsion polymerization. Then, by the method of mass polymerization, we scatter different proportion of those particles onto the monomers of MMA to create particle toughened PMMA and test the thermal stability, mechanical properties and other characteristics of the particle toughened PMMA. The result shows that the particle toughened PMMA we create have an enhancement in toughness and further increase its thermal stability.
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Rzayev, Javid. "Controlled free -radical polymerization at high pressures: Synthesis and properties of poly(α-substituted acrylates)." 2004. https://scholarworks.umass.edu/dissertations/AAI3118328.
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The free-radical polymerization of a series of α-substituted acrylic acid derivatives has been achieved by using hydrostatic pressure as a kinetic and thermodynamic driving force. It is shown that conducting polymerization in a range of pressures between 1 and 9 kbar dramatically improves the polymerizabilities of the investigated acrylates, opening the way to the synthesis of high-molecular weight polymers in short reaction times. The polymerizabilities of α-alkylacrylates at ambient pressure, obtained by extrapolation from high-pressure kinetic data, correlate well with Meyer's steric parameters for the relevant α-alkyl group. While the polymerization of α-alkylacrylates with linear alkyl groups proceeded via a vinyl double-bond addition in a traditional way, methyl α-isobutylacrylate polymerized though alternating steps of addition and 1,5-hydrogen transfer from the penultimate unit to provide an isomeric α-branched polymer structure. Structure-property relationships for the synthesized poly(α-substituted acrylates) have been investigated. Increasing the size of the α-alkyl group decreases thermodynamic stability of the poly(α-alkylacrylates), and facilitates their thermal and photo-degradation. Conformational transitions of poly(α-alkylacrylic acid)s in aqueous solutions are shown to be highly dependent on the size of the α-alkyl group. The transition pH can be fine-tuned by adjusting the total hydrophobic content of the polymer via copolymerization of α-alkylacrylic acid with different alkyl substituents. A high-pressure reversible addition-fragmentation chain transfer (HP-RAFT) protocol for controlled/living free-radical polymerization has been developed. It is demonstrated that this HP-RAFT technique can be used to livingly polymerize sterically hindered monomers, such as methyl ethacrylate, to provide polymers with low polydispersities, controlled molecular weights and end-groups. A methodology for the synthesis of well-defined poly(ethacrylic acid) has been developed. The controlled polymerization of polystyrene-methacrylate macromonomers has been achieved by HP-RAFT, providing densely branched comb-like polymers with controlled molecular weight characteristics. The synthesis of linear-comb diblock copolymers is also achievable by this technique. The HP-RAFT polymerization of traditional monomers, such as methyl methacrylate (MMA), has been investigated. It is demonstrated that the methodology allows for the synthesis of ultra-high molecular weight polymers with low polydispersities. The technique was used to obtain well-defined PMMAs with molecular weights of more than one million.
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Huang, Ling-Wei, and 黃凌威. "Synthesis of UV-Curable Urethane Acrylates and Their Application for High Transparency and Blast-resistence Glass Protective Coating." Thesis, 2009. http://ndltd.ncl.edu.tw/handle/26255105588818810665.
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碩士國立臺灣大學
化學工程學研究所
97
In this study, a series of UV-curable urethane acrylate resin, applied as blast resistant film on the glass substrate were developed. This blast resistant film was designed to be able to stick the glass debris when the glass is broken. We could find the influences of structures with different urethane linkage and crosslink density on thermal, optical, and mechanical properties of urethane acrylate. In order to reach better protective effect, the resin must have outstanding adhesion strength to glass and mechanical property. To improve the interaction between resin and glass, the 3-Methacryloxypropyltrimethoxysilane (MSMA) was used to modify glass surface through sol-gel process to form the chemical bonds with the urethane acrylate resins during the UV-curing process. Tensile property of urethane acrylate resin can be improved by blending high toughness PU to form semi-IPNs structure. In other way, we can design and synthesis the resin which has proper density of urethane linkage and crosslink point by changing average molecular weight of urethane acrylate monomer. IBp051kDUA exhibit the best protective effect in the blast-resistance test, and IBp051kDUA-coated glass has about 90% visible light transmittance.
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Lin, Yen-Ting, and 林彥廷. "Synthesis of dimeric acrylates for single component / mixed chiral LC materials and Study of stabilized Blue Phase LCs." Thesis, 2013. http://ndltd.ncl.edu.tw/handle/86162186893583286210.
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碩士國立交通大學
照明與能源光電研究所
102
We synthesize a series of asymmetric bimolecular single component / blending chiral liquid crystal material, and the chemical structures of these compounds were characterized by H1-NMR、EA, and the liquid crystalline phases before and after the illumination polymerization behavior of all compounds were identified from the result of POM. We have successfully synthesized bimolecular acrylate group material A66CB doped with ZLI-4572, S811 and the blue phase are obtained. When A66CB blends 4wt% of ZLI-457 under illuminated polymerization in blue phase, the widest blue phase temperature can be extended to about 21 °C. In addition, single molecule blue phase dimers A66*CB, which have chiral center in the central of molecular, were synthesized. We synthesize the dimer A66*CB with acrylate group that introduced chiral center successfully has the blue-phase range about 3 °C by single component. Using the A66*CB blending 76*CB and RM257 blending 76*CB for comparison and found that when A66*CB blends 76*CB (10:90), there is the widest blue phase temperature range about 5 °C, and after illuminated polymerization, the blue-phase temperature range will increase. The reactive dimer A66*CB and RM257 after illuminated polymerization in blue-phase, we discovered that A66*CB series can stabilize the blue-phase range better than RM257.
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Bagoury, Mohamed al [Verfasser]. "Synthesis of aqueous polymer colloids based on saccharide monomers and alkyl acrylates through emulsion polymerization / von Mohamed al-Bagoury." 2005. http://d-nb.info/974074527/34.
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Huang, Yang-Kai, and 黃揚凱. "Synthesis of Poly(meth)acrylates in Different Type and Topology by (Atom Transfer) Radical Polymerization and Vitrimerization by Introducing Dynamic Covalent Bond of β-Hydroxy Ester Moiety." Thesis, 2019. http://ndltd.ncl.edu.tw/handle/nmyc4t.
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碩士國立中興大學
化學工程學系所
107
In the first part, we synthesized different type random copolymers of P(MMA-r-GMA) and gradient copolymers of P(MMA-grad-GMA) by radical polymerization or atom transfer radical polymerization. We incorporated crossliker, catalyst, and different PGMA amounts of random copolymers/gradient copolymers to obtain PMMA-based vitrimers and access dynamic covalent networks through dynamic covalent bonds (DCBs). Then, we discussed PMMA-based vitrimers’s mechanical property, thermal property and the influence of the different type vitrimers on thermal healing performance. In the second part, we aimed at improving the mechanical properties of PMMA-based vitrimers. We synthesized different topology of triblock copolymers P(MMA-r-GMA)-b-PnBA-b-P(MMA-r-GMA) and hyperbranched-core star-shape copolymers s[P(MMA-r-GMA)-h-P(nBA- co-BPEA)]. These two kinds of copolymers were also prepared to PMMA-based vitrimers. By introducing soft part (i.e., PnBA) and manipulations of polymer topology, we investigated the thermal and mechanical properties. We can also obtain well thermal healing performance and significant improve on the mechanical property which can be reveal from microstructures within the PMMA-based vitrimers.
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Liao, Sheng-che, and 廖聖哲. "Kinetics for Synthesis of n-Butyl Acrylate." Thesis, 2005. http://ndltd.ncl.edu.tw/handle/83931210451270723321.
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碩士國立臺灣科技大學
化學工程系
93
The heterogeneous kinetics and adsorption behavior of butyl acrylate over an acidic cation-exchange resin, Amberlyst 35, were investigated with a packed-bed reactor. The esterification was performed at temperatures between 333.15 K and 360.75 K. Besides changing temperature，we also focused on the effect of different molar ratios and mass diffusion resistance. Finally, the correlation between by-product and adsorption was studied. The equilibrium conversion of acrylic acid was found to increase with increasing both temperature and the composition of feedθB0. The relative adsorption strengths for the reacting species were determined from adsorption experiments. The results indicated that the magnitude of adsorption strengths followed the order of water > acrylic acid > n-butanol > butyl acrylate. The kinetic data were correlated with the quasi-homogeneous, non- idea-quasi-homogeneous, Langmuir-Hinshelwood-Hougen-Waston, and the Eley-Rideal models, while the model parameters were determined. The LHHW model yielded the best representation for the kinetic behavior of liquid-solid catalytic synthesis of butyl acrylate.
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LI, YI SHIOU, and 李易修. "Kinetics Study of Synthesis of Butyl-acrylate." Thesis, 2002. http://ndltd.ncl.edu.tw/handle/82770466618094158170.
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碩士長庚大學
化學工程研究所
90
The esterification of 1-butanol with acrylic acid catalyzed by sulfuric acid in the absence of solvent was studied in a 500cm3 batch stirred reactor. Experiments were carried out with different acid/alcohol mole ratios and different amounts of sulfuric acid in the temperature range of 70 to 90℃ and at 1 atm. It was found that the esterification of 1-butanol with acrylic acid is a reversible reaction and the esterification step follows a first-order rate expression with respect to each component. A kinetic model was proposed to describe such a reversible esterification reaction catalyzed by sulfuric acid. The equilibrium constants were determined from the equilibrium concentrations of each component while the rate constants were calculated by correlating the experimental data with the developed kinetic model.